CN112121825A - 一种Ag/Ag2Mo2O7/WS2异质结光催化材料及其制备方法 - Google Patents
一种Ag/Ag2Mo2O7/WS2异质结光催化材料及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种Ag/Ag2Mo2O7/WS2异质结光催化材料及其制备方法,属于光催化降解有机污染物技术领域。本发明首次通过原位水热法在WS2纳米片表面生长Ag2Mo2O7纳米晶,并通过光化学还原在复合材料的表面掺杂大量的Ag0,从而得到Ag/Ag2Mo2O7/WS2异质结光催化材料。本发明制备得到的Ag/Ag2Mo2O7/WS2异质结光催化材料较Ag2Mo2O7/WS2复合材料、以及商业Ag2Mo2O7和WS2具有更加优越的光催化降解有机污染物的效率,且制备方法简单,产物产出率高,纯度高,具有可观的应用前景。
Description
技术领域
本发明涉及一种Ag/Ag2Mo2O7/WS2异质结光催化材料及其制备方法,属于光催化降解有机污染物技术领域。
背景技术
众多光催化领域的研究成果表明,高活性的光催化材料应该具有与太阳光谱相匹配的光吸收范围,以及高的光生载流子迁移速率。含银的半导体材料由于具有较窄的带隙、较小的电子和空穴有效质量,显示出了良好的光催化活性,成为可见光催化领域研究的热点。这其中,有关于钼酸银的光催化性能的研究却较少,这主要因为钼酸银材料光谱响应范围窄且光生载流子分离效率低。针对这一问题,近来有少量基于钼酸银的复合材料的光催化研究,然而,这些复合材料的合成步骤较为繁琐,且光催化性能都有待进一步提高。
二硫化钨(WS2)是由单层二维WS2纳米片通过范德华力叠加而成的过渡金属硫化物。通过减小WS2纳米片的横向尺寸可以在WS2纳米粒子的边缘产生大量缺陷和活性位点,边缘结构的改变和较强的量子限制效应赋予了二维WS2纳米片独特的电子特性和可调谐的带隙能,从而产生非凡的电学和光学特性。此外,WS2量子点的上转换性质进一步提高了捕光效率最终导致电子空穴对的产生进而促进了光催化的进程。
近年来,已有一些关于金属硫化物与钼酸盐复合的光催化剂,如,Sangeeta等人合成了一种MoS2纳米片修饰的Ag2Mo2O7微米棒复合光催化剂,其在左氧氟沙星的光催化氧化应用中具有高效的光催化活性(“Z-scheme 2D/1D MoS2 nanosheet-decorated Ag2Mo2O7microrods for efficient catalytic oxidation of levofloxacin”,ChemicalEngineering Journal 373 (2019) 31–43);Jiyun Gao等人用剥离产生的少层WS2为衬底通过一种简单的溶剂热生长法制备出WS2/Bi2MoO6异质结光催化剂,实验结果表明层状WS2纳米片与Bi2MoO6纳米片之间存在良好的界面效应,在可见光照射下,WS2/Bi2MoO6复合材料对罗丹明B有良好的光催化降解活性(“Facile Synthesis of Heterostructured WS2/Bi2MoO6 as High-Performance Visible-Light-Driven Photocatalysts”, NanoscaleResearch Letters (2017) 12:377)。上述复合光催化材料的光催化活性仍有望提高。
发明内容
本发明的目的之一在于提供一种Ag/Ag2Mo2O7/WS2异质结光催化材料,其中Ag2Mo2O7原位生长于WS2纳米片的表面,Ag以Ag0形式掺杂于Ag2Mo2O7表面,Ag、Ag2Mo2O7、WS2的质量比为0.01-0.2:0.5-4:1。
进一步的,所述Ag、Ag2Mo2O7、WS2的质量比优选为0.05-0.15:1-3:1。
进一步的,所述WS2纳米片的厚度为1-40nm。
本发明的目的之二在于提供一种Ag/Ag2Mo2O7/WS2异质结光催化材料的制备方法,包括如下的制备步骤:
(1)称取1-2g的WS2粉末溶于100-200mL乙醇与水的混合溶液中,搅拌均匀后超声2-10h,所得的分散液经1000-3000rmp转速离心机离心分离,取上清液即为经剥离的WS2纳米片悬浮液;
(2)分别配制0.01-0.2mol/L的AgNO3和0.01-0.15mol/L的Na2MoO4·2H2O水溶液,并依次滴加至步骤(1)中的WS2纳米片悬浮液中,使得混合体系中的Ag、Mo、W的摩尔比为0.5-4:0.5-4:1,加入1-3mL聚乙烯吡咯烷酮作为稳定剂,持续搅拌0.5-1h,加入硝酸以调节体系pH为2-4,继续搅拌10-30min,将所得混合液转移入聚四氟乙烯内衬的不锈钢反应釜中,升温至120-160℃水热反应12-24h,待反应结束后,自然冷却至室温,过滤,洗涤得到异质结Ag2Mo2O7/WS2复合材料;
(3)将步骤(2)所得复合材料研磨并平铺于表面皿上,用150 W的金卤灯光照 1-2h,将复合材料表面的银离子还原为Ag0,从而得到所述Ag/Ag2Mo2O7/WS2异质结光催化材料。
进一步的,所述步骤(1)中的离心转速优选为2000-2500rmp。
进一步的,所述步骤(2)中的水热反应的温度优选为130-150℃,时间优选为15-20h。
本发明首次通过原位水热法在WS2纳米片表面生长Ag2Mo2O7纳米晶,WS2纳米片和Ag2Mo2O7纳米晶在结合界面形成交错带隙异质结结构,有效促进光生电荷载流子的分离和迁移,从而减少电子-空穴对的复合率,大量的电子和空穴可以分别参与光氧化还原反应,促进光催化效率。进一步的,经光化学还原后,复合材料的表面掺杂了大量的Ag0,上述Ag0粒子具有很强的可见光吸收能力,并在吸收光后在表面发生等离子体共振效应,从而提升复合材料的光催化性能。
本发明制备得到的Ag/Ag2Mo2O7/WS2异质结光催化材料较Ag2Mo2O7/WS2复合材料、以及商业Ag2Mo2O7和WS2具有更加优越的光催化降解有机污染物的效率,且制备方法简单,产物产出率高,纯度高,具有可观的应用前景。
附图说明
图1示出了本发明制备的Ag/Ag2Mo2O7/WS2异质结光催化材料的XRD图谱。
图2示出了本发明制备的Ag/Ag2Mo2O7/WS2异质结光催化材料对罗丹明B的降解效率。
具体实施方式
下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1
(1)称取1.5g的WS2粉末溶于150mL乙醇与水的混合溶液中,搅拌均匀后超声5h,所得的分散液经2400rmp转速离心机离心分离,取上清液即为经剥离的WS2纳米片悬浮液;
(2)分别配制0.1mol/L的AgNO3和0.1mol/L的Na2MoO4·2H2O水溶液,并依次滴加至步骤(1)中的WS2纳米片悬浮液中,使得混合体系中的Ag、Mo、W的摩尔比为2:2:1,加入2mL聚乙烯吡咯烷酮作为稳定剂,持续搅拌0.6h,加入硝酸以调节体系pH为3,继续搅拌20min,将所得混合液转移入聚四氟乙烯内衬的不锈钢反应釜中,升温至140℃水热反应20h,待反应结束后,自然冷却至室温,过滤,洗涤得到异质结Ag2Mo2O7/WS2复合材料;
(3)将步骤(2)所得复合材料研磨并平铺于表面皿上,用150 W的金卤灯光照 2h,将复合材料表面的银离子还原为Ag0,从而得到本实施例的Ag/Ag2Mo2O7/WS2异质结光催化材料,其中,Ag、Ag2Mo2O7、WS2的质量比为0.1:2.2:1;图1为本实施例产物的XRD图谱,由XRD图可以看出本实施例的复合材料显示出了明显的Ag、Ag2Mo2O7、WS2的特征衍射峰,说明本发明成功合成了三元复合体系,且无明显杂质。
实施例2
(1)称取2g的WS2粉末溶于150mL乙醇与水的混合溶液中,搅拌均匀后超声8h,所得的分散液经2000rmp转速离心机离心分离,取上清液即为经剥离的WS2纳米片悬浮液;
(2)分别配制0.1mol/L的AgNO3和0.1mol/L的Na2MoO4·2H2O水溶液,并依次滴加至步骤(1)中的WS2纳米片悬浮液中,使得混合体系中的Ag、Mo、W的摩尔比为1.7:1.7:1,加入2mL聚乙烯吡咯烷酮作为稳定剂,持续搅拌0.6h,加入硝酸以调节体系pH为3,继续搅拌30min,将所得混合液转移入聚四氟乙烯内衬的不锈钢反应釜中,升温至130℃水热反应18h,待反应结束后,自然冷却至室温,过滤,洗涤得到异质结Ag2Mo2O7/WS2复合材料;
(3)将步骤(2)所得复合材料研磨并平铺于表面皿上,用150 W的金卤灯光照 2h,将复合材料表面的银离子还原为Ag0,从而得到本实施例的Ag/Ag2Mo2O7/WS2异质结光催化材料,其中,Ag、Ag2Mo2O7、WS2的质量比为0.12:1.9:1。
实施例3
配制100ml 0.1mM的罗丹明B水溶液作为模拟有机污染物废水,将5mg光催化材料加入到上述罗丹明B水溶液中,避光搅拌2h达到吸附平衡。以300W的氙灯作为光源,通过紫外过滤光片得到可见光,对上述体系进行照射1h,进行光催化降解测试;为了进行对比,对Ag2Mo2O7、WS2、Ag2Mo2O7/WS2复合材料亦进行上述光催化降解测试;图2即示出了本发明实施例1经步骤(1)、(2)制备得到的Ag2Mo2O7/WS2复合材料、经步骤(1)-(3)制备得到的Ag/Ag2Mo2O7/WS2异质结光催化材料以及商业Ag2Mo2O7和WS2对罗丹明B的光催化降解效率,由图2可以明显看出,本发明得到的Ag/Ag2Mo2O7/WS2异质结光催化材料较其余对比光催化材料显示出了明显优越的催化降解性能,具有可观的应用前景。
此外,应当理解,虽然本说明书按照实施方式加光催化以描述,但并非每个实施方式仅包含一个独立的技术方案,说明书的这种叙述方式仅仅是为清楚起见,本领域技术人员应当将说明书作为一个整体,各实施例中的技术方案也可以经适当组合,形成本领域技术人员可以理解的其他实施方式。
Claims (6)
1.一种Ag/Ag2Mo2O7/WS2异质结光催化材料,其特征在于,其中Ag2Mo2O7原位生长于WS2纳米片的表面,Ag以Ag0形式掺杂于Ag2Mo2O7表面,Ag、Ag2Mo2O7、WS2的质量比为0.01-0.2:0.5-4:1。
2.根据权利要求1所述的光催化材料,其特征在于,所述Ag、Ag2Mo2O7、WS2的质量比优选为0.05-0.15:1-3:1。
3.根据权利要求1所述的光催化材料,其特征在于,所述WS2纳米片的厚度为1-40nm。
4.根据权利要求1-3任一所述的一种Ag/Ag2Mo2O7/WS2异质结光催化材料的制备方法,其特征在于,包括如下的制备步骤:
(1)称取1-2g的WS2粉末溶于100-200mL乙醇与水的混合溶液中,搅拌均匀后超声2-10h,所得的分散液经1000-3000rmp转速离心机离心分离,取上清液即为经剥离的WS2纳米片悬浮液;
(2)分别配制0.01-0.2mol/L的AgNO3和0.01-0.15mol/L的Na2MoO4·2H2O水溶液,并依次滴加至步骤(1)中的WS2纳米片悬浮液中,使得混合体系中的Ag、Mo、W的摩尔比为0.5-4:0.5-4:1,加入1-3mL聚乙烯吡咯烷酮作为稳定剂,持续搅拌0.5-1h,加入硝酸以调节体系pH为2-4,继续搅拌10-30min,将所得混合液转移入聚四氟乙烯内衬的不锈钢反应釜中,升温至120-160℃水热反应12-24h,待反应结束后,自然冷却至室温,过滤,洗涤得到异质结Ag2Mo2O7/WS2复合材料;
(3)将步骤(2)所得复合材料研磨并平铺于表面皿上,用150 W的金卤灯光照 1-2h,将复合材料表面的银离子还原为Ag0,从而得到所述Ag/Ag2Mo2O7/WS2异质结光催化材料。
5.根据权利要求4所述的制备方法,其特征在于,所述步骤(1)中的离心转速优选为2000-2500rmp。
6.根据权利要求4所述的制备方法,其特征在于,所述步骤(2)中的水热反应的温度优选为130-150℃,时间优选为15-20h。
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